CN107958760A - A kind of rare earth permanent-magnetic material and preparation method thereof - Google Patents

A kind of rare earth permanent-magnetic material and preparation method thereof Download PDF

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CN107958760A
CN107958760A CN201610901011.6A CN201610901011A CN107958760A CN 107958760 A CN107958760 A CN 107958760A CN 201610901011 A CN201610901011 A CN 201610901011A CN 107958760 A CN107958760 A CN 107958760A
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rare earth
powder
magnetic
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preparation
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CN107958760B (en
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陈侃
郭帅
范晓东
丁广飞
陈仁杰
闫阿儒
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/32—Ferrous alloys, e.g. steel alloys containing chromium with boron

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Power Engineering (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The present invention relates to a kind of preparation method of rare earth permanent-magnetic material, it comprises the following steps：(1) master alloying magnetic powder and auxiliary alloyed powder are provided respectively, wherein the chemical formula of the master alloying magnetic powder is [(PrrNd1‑r)xMM1‑x)]aTmbBcFe1‑a‑b‑c, MM is at least one of high abundance rare earth La, Ce, and the one or more in Tm Fe, Ga, Co, Cu, Nb, Al, Zr element, the chemical formula of the auxiliary alloyed powder is Cey(FedM1‑d)1‑y, y, d are the mass percentage of corresponding element, the one or more in M Cu, Al, Ga, Co, Ni；(2) the master alloying magnetic powder is uniformly mixed with the auxiliary alloyed powder to obtain mixing magnetic powder, wherein, the mass percent described in the mixing magnetic powder shared by auxiliary alloyed powder is 1%~5%；(3) the mixing magnetic powder is subjected to oriented moulding, sintering and temper successively, obtains rare earth permanent-magnetic material.The present invention also provides a kind of rare earth permanent-magnetic material obtained using above-mentioned preparation method.

Description

A kind of rare earth permanent-magnetic material and preparation method thereof
Technical field
The present invention relates to a kind of rare earth permanent-magnetic material and preparation method thereof.
Background technology
Rare earth permanent-magnetic material is the intermetallic compound formed using thulium and magnesium-yttrium-transition metal as matrix Permanent-magnet material.Nd-Fe-B permanent magnet material (also referred to as NdFeB permanent-magnet materials) has excellent magnetic characteristic, is widely used to social life The fields such as production, life and national defence and space flight, become the critical function material of support social progress.In NdFeB permanent-magnet materials, The cost of rare earth Nd accounts for more than the 90% of the cost of raw material.With industrial expansion and social progress, Nd-Fe-B permanent magnetism materials The usage amount of material increases year by year, and production cost is also higher and higher.Moreover, the rare earth often added in Nd-Fe-B permanent-magnet materials Member is known as praseodymium (Pr), dysprosium (Dy), terbium (Tb), still, these rare earth metals particularly heavy rare earth proportion in rare earth resources Few, resource shortage is expensive.Therefore, much work as without heavy rare earth or few had become with heavy rare earth with to reduce the research of cost The research emphasis in preceding field.
In the recovery process of Rare Earth Mine, primary Rare Earth Mine obtains norium (Misch by chemical treatment Metal), mischmetal goes out lanthanum (La), cerium (Ce) and the praseodymium (Pr) containing cerium, neodymium (Nd) enriched substance by extract and separate, then passes through Extract and separate obtains Pr and Nd.While Pr, Nd metal smelting, these lanthanums (La), cerium (Ce) metal are also refined at the same time, production Amount is very high, but its price is but far below metals such as praseodymium, neodymiums.And the extensive application of praseodymium neodymium alloy causes the big of the metals such as lanthanum, cerium Amount is overstock.
The utilization of sintered permanent magnet is prepared for high abundance rare earth at present, mainly still concentrates on the stage that technique is groped. For example in patent application CN1035737A disclosed in China, by La, Ce part substitution Nd by the way of direct melting, obtain A kind of cheap Nd-La, Ce-Fe-B magnets, but magnet performance deteriorate obvious.
The content of the invention
In view of this, it is necessory to provide, a kind of cost is relatively low and the preferable rare earth permanent-magnetic material of magnetic property and its preparation side Method.
The present invention provides a kind of preparation method of rare earth permanent-magnetic material, it comprises the following steps：
(1) master alloying magnetic powder and auxiliary alloyed powder are provided respectively, wherein the chemical formula of the master alloying magnetic powder is [(PrrNd1-r)xMM1-x)]aTmbBcFe1-a-b-c, r, x, a, b, c are the mass percentage of corresponding element, and 0≤r≤1,0≤x ≤ 1,28≤a≤33,0≤b≤5,0.85≤c≤1.5, MM are high abundance rare earth La, at least one of Ce, Tm Fe, Ga, One or more in Co, Cu, Nb, Al, Zr element, the chemical formula of the auxiliary alloyed powder is Cey(FedM1-d)1-y, y, d are correspondence The mass percentage of element, and 0.5≤y≤1, wherein 0≤d≤1, M are the one or more in Cu, Al, Ga, Co, Ni；
(2) the master alloying magnetic powder is uniformly mixed with the auxiliary alloyed powder to obtain mixing magnetic powder, wherein, in the mixing Mass percent described in magnetic powder shared by auxiliary alloyed powder is 1%~5%；
(3) the mixing magnetic powder is subjected to oriented moulding, sintering and temper successively, obtains rare earth permanent-magnetic material.
Wherein, the mass percent described in the mixing magnetic powder shared by auxiliary alloyed powder is 1%~3%.
Wherein, the preparation method of master alloying magnetic powder is as follows described in step (1)：
First, according to [(PrrNd1-r)xMM1-x)]aTmbBcFe1-a-b-cProportioning configuration raw material, and be put into rapid hardening furnace melt Refine master alloying, obtain master alloying rapid-hardening flake, wherein the fusion process carries out under an inert atmosphere, smelting temperature for 1300 DEG C~ 1450 DEG C, copper roller rotating speed is 1m/s~1.5m/s during melting, obtains the master alloying rapid-hardening flake that average thickness is 0.1mm~0.5mm；
Then, by the master alloying rapid-hardening flake carry out successively hydrogen break, airflow milling, it is 1 μm~5 μm of master to obtain average grain diameter Alloy magnetic powder.
Wherein, the preparation method of auxiliary alloyed powder is as follows described in step (1)：
First, according to Cey(FedM1-d)1-yProportioning configuration raw material, and be put into the auxiliary alloy of melting in rapid hardening furnace, obtain auxiliary conjunction Golden ingot casting；
Then, the auxiliary alloy cast ingot is carried out hydrogen successively to break to obtain auxiliary alloy coarse crushing powder；
Finally, ball milling or airflow milling are carried out to the auxiliary alloy coarse crushing powder, obtains the auxiliary alloy that average grain diameter is less than 2 μm Powder.
Wherein, the process of oriented moulding is specially described in step (3)：Magnetic powder oriented moulding in magnetic field will be mixed, Blank magnet is obtained, then by isostatic pressed is handled in hydraulic press after obtained blank magnet Vacuum Package.
Wherein, the process sintered described in step (3) is specially：By the blank magnet obtained after oriented moulding in vacuum Sintered in sintering furnace, wherein sintering temperature be 950 DEG C~1050 DEG C, sintering time for 1 it is small when~6 it is small when.
Wherein, the process of temper is specially described in step (3)：The sintered magnet obtained after sintering is subjected to heat Processing, wherein the temperature being heat-treated is 400 DEG C~800 DEG C, time of heat treatment for 1 it is small when~6 it is small when.
The present invention also provides a kind of rare earth permanent-magnetic material obtained using above-mentioned preparation method, the rare earth permanent-magnetic material exists Magnet grain boundaries form (Ce, RE)56Fe44Grain-Boundary Phase, wherein RE is at least one of for La, Pr, Nd.
Compared with prior art, rare earth permanent-magnetic material of the present invention and preparation method thereof has the following advantages：
First, by introducing ferrocerium Kiev alloyed powder, change Grain-Boundary Phase the Nomenclature Composition and Structure of Complexes so that sintered magnet is brilliant after optimization Boundary has the eutectic reaction fusion temperature lower compared with conventional magnet crystal boundary, improves the mobility of crystal boundary, and thin area's crystal boundary thickness increases Add, go magnetic coupling interaction to strengthen between main phase grain.
Second, the controllable distribution of high abundance rare-earth element cerium and lanthanum inside magnet of introducing of ferrocerium Kiev alloyed powder and Cheng Xiang, is allowed to integrated distribution in magnet grain boundaries, forms a kind of RE56Fe44(wt.%) Grain-Boundary Phase, increase grain boundaries are non-magnetic Property phase volume fraction, therefore magnetic reversal farmland forming core can be suppressed during demagnetization, hinder the migration of magnetic reversal domain wall, significantly Lift the coercivity of the rare earth permanent-magnetic material.
3rd, the introducing of ferrocerium Kiev alloyed powder can inhibit the diffusion of high abundance rare-earth element cerium and lanthanum in crystal grain, protect Hold high saturation and magnetic intensity and the high anisotropy field of hard magnetic phase, so as to get rare earth permanent-magnetic material there is excellent comprehensive magnetic Energy.
In addition, high abundance rare earth La, Ce parts replacement Pr are used in raw materials used middle master alloying magnetic powder, Nd rare earth elements, It is few with resource consumption to the energy, promote high abundance rare earth element balance and efficient utilization, while material cost can be substantially reduced, Alleviate environmental pollution.
Brief description of the drawings
Fig. 1 is that (wherein+1 is poor iron for the backscattered electron shape appearance figure of 1 obtained rare earth permanent-magnetic material of the embodiment of the present invention Grain-Boundary Phase ,+2 be rich iron Grain-Boundary Phase, and+3 be main phase grain).
Specific examples below will combine above-mentioned attached drawing and further illustrate the present invention.
Embodiment
Rare earth permanent-magnetic material provided by the invention and preparation method thereof is described further below with reference to attached drawing.
The present invention provides a kind of preparation method of rare earth permanent-magnetic material, it includes following steps：
S1, provides master alloying magnetic powder and auxiliary alloyed powder, wherein the chemical formula of the master alloying magnetic powder is respectively [(PrrNd1-r)xMM1-x)]aTmbBcFe1-a-b-c, r, x, a, b, c are the mass percentage of corresponding element, and 0≤r≤1,0≤x ≤ 1,28≤a≤33,0≤b≤5,0.85≤c≤1.5, MM are high abundance rare earth La, at least one of Ce, Tm Fe, One or more in Ga, Co, Cu, Nb, Al, Zr element, the chemical formula of the auxiliary alloyed powder is Cey(FedM1-d)1-y, y, d are The mass percentage of corresponding element, and 0.5≤y≤1, wherein 0≤d≤1, M are one kind or several in Cu, Al, Ga, Co, Ni Kind；
S2, the master alloying magnetic powder is uniformly mixed with the auxiliary alloyed powder to obtain mixing magnetic powder, wherein, in the mixing Mass percent described in magnetic powder shared by auxiliary alloyed powder is 1%~5%；And
S3, carries out oriented moulding, sintering and temper by the mixing magnetic powder, obtains rare earth permanent-magnetic material successively.
In step sl, parameter r, x, a, b, c in the chemical formula of the master alloying magnetic powder can use following preferred scope： 0.4≤x≤1,29≤a≤31,0≤b≤5,0.9≤c≤1.5.
The master alloying magnetic powder can be prepared by the following preparation method：
S111, according to [(PrrNd1-r)xMM1-x)]aTmbBcFe1-a-b-cProportioning configuration raw material, and be put into rapid hardening furnace melt Refine master alloying, obtain master alloying rapid-hardening flake, wherein the fusion process carries out under an inert atmosphere, smelting temperature for 1300 DEG C~ 1450 DEG C, copper roller rotating speed is 1m/s~1.5m/s during melting, obtains the master alloying rapid-hardening flake that average thickness is 0.1mm~0.5mm；
S112, by the master alloying rapid-hardening flake carry out successively hydrogen break, airflow milling, it is 1 μm~5 μm of master to obtain average grain diameter Alloy magnetic powder.
Wherein described inert atmosphere refers to the atmosphere such as nitrogen, argon gas, neon, Krypton.
Parameter y, d in the chemical formula of the auxiliary alloyed powder can use following preferred scope：0.8≤y≤1,0.5≤d≤ 1。
The preparation method of the auxiliary alloyed powder is as follows：
S121, according to Cey(FedM1-d)1-yProportioning configuration raw material, and be put into the auxiliary alloy of melting in rapid hardening furnace, obtain auxiliary conjunction Golden ingot casting；
S122, carries out hydrogen by the auxiliary alloy cast ingot and breaks to obtain auxiliary alloy coarse crushing powder successively；
S123, carries out ball milling or airflow milling to the auxiliary alloy coarse crushing powder, obtains the auxiliary alloy that average grain diameter is less than 2 μm Powder.
In step s 2, by the way that the master alloying magnetic powder is mixed with the auxiliary alloyed powder so that the auxiliary alloyed powder is equal It is even to be distributed in the master alloying magnetic powder.The mixing can carry out in three-dimensional material mixer.It is auxiliary described in the mixing magnetic powder Mass ratio shared by alloyed powder is preferably 1%~3%.
In step s3, the process of the oriented moulding is specially：Magnetic powder oriented moulding in magnetic field will be mixed, obtains hair Base magnet, then by isostatic pressed is handled in hydraulic press after obtained blank magnet Vacuum Package.
The process of the sintering is specially：The blank magnet obtained after oriented moulding is sintered in vacuum sintering furnace, its Middle sintering temperature be 950 DEG C~1050 DEG C, sintering time for 1 it is small when~6 it is small when.Preferably, sintering temperature is 980 DEG C~1010 DEG C, sintering time for 2 it is small when~4 it is small when.
The process of the temper is specially：The sintered magnet obtained after sintering is heat-treated, wherein being heat-treated Temperature be 400 DEG C~800 DEG C, time of heat treatment for 1 it is small when~6 it is small when.Preferably, the temperature of heat treatment for 500 DEG C~ 700 DEG C, time of heat treatment for 2 it is small when~4 it is small when.
The present invention also provides a kind of rare earth permanent-magnetic material obtained using above-mentioned preparation method.The rare earth permanent-magnetic material exists Magnet grain boundaries form (Ce, RE)56Fe44(wt%) Grain-Boundary Phase, wherein RE are at least one of La, Pr, Nd.Need It is bright, (Ce, the RE) of formation56Fe44Grain-Boundary Phase is Approximation Quality ratio.
Compared with prior art, rare earth permanent-magnetic material of the present invention and preparation method thereof has the following advantages：
First, by introducing ferrocerium Kiev alloyed powder, change Grain-Boundary Phase the Nomenclature Composition and Structure of Complexes so that sintered magnet is brilliant after optimization Boundary has the eutectic reaction fusion temperature lower compared with conventional magnet crystal boundary, improves the mobility of crystal boundary, and thin area's crystal boundary thickness increases Add, go magnetic coupling interaction to strengthen between main phase grain.
Second, the controllable distribution of high abundance rare-earth element cerium and lanthanum inside magnet of introducing of ferrocerium Kiev alloyed powder and Cheng Xiang, is allowed to integrated distribution in magnet grain boundaries, forms a kind of RE56Fe44(wt.%) Grain-Boundary Phase, increase grain boundaries are non magnetic The volume fraction of phase, therefore magnetic reversal farmland forming core can be suppressed during demagnetization, the migration of magnetic reversal domain wall is hindered, is carried significantly Rise the coercivity of the rare earth permanent-magnetic material.
3rd, the introducing of ferrocerium Kiev alloyed powder can inhibit the diffusion of high abundance rare-earth element cerium and lanthanum in crystal grain, protect Hold high saturation and magnetic intensity and the high anisotropy field of hard magnetic phase, so as to get rare earth permanent-magnetic material there is excellent comprehensive magnetic Energy.
In addition, high abundance rare earth La, Ce parts replacement Pr are used in raw materials used middle master alloying magnetic powder, Nd rare earth elements, It is few with resource consumption to the energy, promote high abundance rare earth element balance and efficient utilization, while material cost can be substantially reduced, Alleviate environmental pollution.
Hereinafter, will further illustrate in conjunction with specific embodiments.
Embodiment (1)
According to [(Pr0.2Nd0.8)0.72Ce0.28]30.5Al0.2Cu0.1Ga0.1Fe68.1B1Proportioning carries out proportioning master alloying raw material.Will Proportioned master alloying is put into melting in rapid hardening furnace, wherein smelting temperature control copper roller at 1350 DEG C, melting after polishing Rotating speed is maintained at 1.2m/s.The master alloying rapid-hardening flake that average thickness is 0.3mm~0.5mm is obtained by strip casting.It will obtain Master alloying rapid-hardening flake be placed in hydrogen broken furnace, be flushed with hydrogen broken, obtain master alloying coarse crushing powder, then will obtain master alloying and slightly break Comminuted powder continues to crush in the airflow mill that nitrogen is protected, and the master alloying air-flow for obtaining average grain diameter at 2 μm~3 μm is milled End.
According to Ce92Fe8Proportioning carry out matching auxiliary alloy raw material.Auxiliary alloy polishing after proportioning is clean, it is placed in vacuum Melting obtains auxiliary alloy cast ingot in induction heater.Obtained auxiliary alloy cast ingot is placed in suction hydrogen in hydrogen broken furnace to crush, is obtained auxiliary Alloy coarse crushing powder.For the consideration of control oxygen, under nitrogen environmental protection, auxiliary alloy coarse crushing powder is inserted into ball grinder In, according to 1:10 ratio of grinding media to material, carries out mechanical ball mill processing to auxiliary alloy coarse crushing powder, obtains auxiliary alloy powder.
The auxiliary alloy powder that the master alloying airflow milling powder homogenous quantities fraction that mass fraction is 99% is 1% is uniformly mixed The oriented moulding in magnetic field afterwards, obtains blank magnet.By after obtained blank magnet Vacuum Package in hydraulic press at isostatic pressed Reason.
Obtained magnet blank is sintered in vacuum sintering furnace, wherein 1005 DEG C of sintering temperature, when sintering duration 2 is small. Obtained sintered magnet is carried out to be thermally treated resulting in rare earth permanent-magnetic material, wherein 650 DEG C of temperature, when tempering duration 2 is small.
Obtained rare earth permanent-magnetic material is tested at room temperature using the permanent magnetism B-H hysteresiscopes of NIM-500C types Magnetic property, test result test result are shown in Table 1.
Morphology analysis also is carried out to obtained rare earth permanent-magnetic material.Referring to Fig. 1, wherein+1 is poor iron crystal boundary Phase ,+2 (Ce, the RE) newly to be formed56Fe44Rich iron Grain-Boundary Phase ,+3 be main phase grain.
Embodiment (2)
Embodiment (2) prepare rare earth permanent-magnetic material process and embodiment (1) it is essentially identical, difference is, by matter The auxiliary alloy powder mixing that the master alloying airflow milling powder homogenous quantities fraction that amount fraction is 97% is 3%, and in sintering process Sintering temperature is 1000 DEG C.
Obtained rare earth permanent-magnetic material is subjected to test magnetic property at room temperature, test result test result is shown in Table 1.
Embodiment (3)
Embodiment (3) prepare rare earth permanent-magnetic material process and embodiment (1) it is essentially identical, difference is, by matter The auxiliary alloy powder mixing that the master alloying airflow milling powder homogenous quantities fraction that amount fraction is 95% is 5%；And in sintering process Sintering temperature is 1000 DEG C；And heat treatment temperature is 700 DEG C in tempering process.
Obtained rare earth permanent-magnetic material is subjected to test magnetic property at room temperature, test result is shown in Table 1.
Comparative example
Comparative example prepare rare earth permanent-magnetic material process and embodiment (1) it is essentially identical, difference is, is added without auxiliary Alloyed powder.
Obtained rare earth permanent-magnetic material is subjected to test magnetic property at room temperature, test result test result is shown in Table 1.
The magnetic property of rare earth permanent-magnetic material made from 1 embodiment 1 to 3 of table
Br(T) Hc(kA/m) (BH)max(kJ/m3)
Embodiment 1 1.246 1118.8 277.5
Embodiment 2 1.206 1104.8 253.9
Embodiment 3 1.144 999.9 214.7
Comparative example 1.246 1007.1 268.5
By table 1 as it can be seen that for comparative example, embodiment 1 to 3 is ensureing institute by introducing suitable auxiliary alloyed powder While the remanent magnetism unobvious of obtained rare earth permanent-magnetic material decline, and its coercivity is got a promotion.
The explanation of above example is only intended to help to understand method and its core concept of the invention.It should be pointed out that pair For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out Some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or use the present invention. A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention The embodiments shown herein is not intended to be limited to, and is to fit to and the principles and novel features disclosed herein phase one The most wide scope caused.

Claims (8)

1. a kind of preparation method of rare earth permanent-magnetic material, it comprises the following steps：
(1) master alloying magnetic powder and auxiliary alloyed powder are provided respectively, wherein the chemical formula of the master alloying magnetic powder is [(PrrNd1-r)xMM1-x)]aTmbBcFe1-a-b-c, r, x, a, b, c are the mass percentage of corresponding element, and 0≤r≤1,0≤x≤1,28≤a ≤ 33,0≤b≤5,0.85≤c≤1.5, MM are high abundance rare earth La, at least one of Ce, Tm Fe, Ga, Co, Cu, Nb, One or more in Al, Zr element, the chemical formula of the auxiliary alloyed powder is Cey(FedM1-d)1-y, y, d are the matter of corresponding element Percentage composition, and 0.5≤y≤1 are measured, 0≤d≤1, wherein M are the one or more in Cu, Al, Ga, Co, Ni；
(2) the master alloying magnetic powder is uniformly mixed with the auxiliary alloyed powder to obtain mixing magnetic powder, wherein, in the mixing magnetic powder Described in mass percent shared by auxiliary alloyed powder be 1%~5%；
(3) the mixing magnetic powder is subjected to oriented moulding, sintering and temper successively, obtains rare earth permanent-magnetic material.
2. the preparation method of rare earth permanent-magnetic material as claimed in claim 1, it is characterised in that described in the mixing magnetic powder Mass percent shared by auxiliary alloyed powder is 1%~3%.
3. the preparation method of rare earth permanent-magnetic material as claimed in claim 1, it is characterised in that the main conjunction described in step (1) The preparation method of golden magnetic powder is as follows：
First, according to [(PrrNd1-r)xMM1-x)]aTmbBcFe1-a-b-cProportioning configuration raw material, and be put into melting master in rapid hardening furnace Alloy, obtains master alloying rapid-hardening flake, wherein the fusion process carries out under an inert atmosphere, smelting temperature is 1300 DEG C~1450 DEG C, copper roller rotating speed is 1m/s~1.5m/s during melting, obtains the master alloying rapid-hardening flake that average thickness is 0.1mm~0.5mm；
Then, by the master alloying rapid-hardening flake carry out successively hydrogen break, airflow milling, it is 1 μm~5 μm of master alloying to obtain average grain diameter Magnetic powder.
4. the preparation method of rare earth permanent-magnetic material as claimed in claim 1, it is characterised in that the auxiliary conjunction described in step (1) The preparation method of bronze is as follows：
First, according to Cey(FedM1-d)1-yProportioning configuration raw material, and be put into the auxiliary alloy of melting in rapid hardening furnace, obtain auxiliary alloy casting Ingot；
Then, the auxiliary alloy cast ingot is carried out hydrogen successively to break to obtain auxiliary alloy coarse crushing powder；
Finally, ball milling or airflow milling are carried out to the auxiliary alloy coarse crushing powder, obtains the auxiliary alloyed powder that average grain diameter is less than 2 μm.
5. the preparation method of rare earth permanent-magnetic material as claimed in claim 1, it is characterised in that be orientated described in step (3) Molding process is specially：Magnetic powder oriented moulding in magnetic field will be mixed, obtains blank magnet, then obtained blank magnet is true Isostatic pressed is handled in hydraulic press after sky encapsulation.
6. the preparation method of rare earth permanent-magnetic material as claimed in claim 1, it is characterised in that sintered described in step (3) Process be specially：The blank magnet obtained after oriented moulding is sintered in vacuum sintering furnace, wherein sintering temperature is 950 DEG C ~1050 DEG C, sintering time for 1 it is small when~6 it is small when.
7. the preparation method of rare earth permanent-magnetic material as claimed in claim 1, it is characterised in that be tempered described in step (3) The process of processing is specially：The sintered magnet obtained after sintering is heat-treated, wherein the temperature being heat-treated for 400 DEG C~ 800 DEG C, time of heat treatment for 1 it is small when~6 it is small when.
8. a kind of rare earth permanent-magnetic material obtained using the preparation method as described in claim 1 to 7, it is characterised in that described dilute Native permanent-magnet material forms (Ce, RE) in magnet grain boundaries56Fe44Grain-Boundary Phase, wherein RE is at least one of for La, Pr, Nd.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108987016A (en) * 2018-07-13 2018-12-11 杭州电子科技大学 A kind of preparation process of nano-crystal neodymium iron boron magnetic body
CN109468520A (en) * 2018-10-24 2019-03-15 京磁材料科技股份有限公司 The method of supersonic oscillations melting Nd Fe B alloys
WO2020133341A1 (en) * 2018-12-29 2020-07-02 三环瓦克华（北京）磁性器件有限公司 Rare-earth magnet, magnet having sputtered rare earth, and magnet having diffused rare earth, and preparation method
CN111957979A (en) * 2020-07-10 2020-11-20 瑞声科技（南京）有限公司 Auxiliary alloy powder for permanent magnet material, preparation method of auxiliary alloy powder and permanent magnet material
CN113549813A (en) * 2021-07-22 2021-10-26 江西理工大学 Preparation method of main-auxiliary phase nanocrystalline high-abundance rare earth permanent magnet material
WO2024113657A1 (en) * 2022-11-30 2024-06-06 福建省金龙稀土股份有限公司 Magnetic steel containing high-abundance rare earth elements, preparation method therefor, and use thereof

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Publication number Priority date Publication date Assignee Title
CN108987016A (en) * 2018-07-13 2018-12-11 杭州电子科技大学 A kind of preparation process of nano-crystal neodymium iron boron magnetic body
CN108987016B (en) * 2018-07-13 2021-06-18 杭州电子科技大学 Preparation process of nanocrystalline neodymium-iron-boron magnet
CN109468520A (en) * 2018-10-24 2019-03-15 京磁材料科技股份有限公司 The method of supersonic oscillations melting Nd Fe B alloys
CN109468520B (en) * 2018-10-24 2020-07-21 京磁材料科技股份有限公司 Method for smelting neodymium iron boron alloy by ultrasonic oscillation
WO2020133341A1 (en) * 2018-12-29 2020-07-02 三环瓦克华（北京）磁性器件有限公司 Rare-earth magnet, magnet having sputtered rare earth, and magnet having diffused rare earth, and preparation method
CN111957979A (en) * 2020-07-10 2020-11-20 瑞声科技（南京）有限公司 Auxiliary alloy powder for permanent magnet material, preparation method of auxiliary alloy powder and permanent magnet material
CN111957979B (en) * 2020-07-10 2023-02-28 瑞声科技（南京）有限公司 Auxiliary alloy powder for permanent magnet material, preparation method of auxiliary alloy powder and permanent magnet material
CN113549813A (en) * 2021-07-22 2021-10-26 江西理工大学 Preparation method of main-auxiliary phase nanocrystalline high-abundance rare earth permanent magnet material
WO2024113657A1 (en) * 2022-11-30 2024-06-06 福建省金龙稀土股份有限公司 Magnetic steel containing high-abundance rare earth elements, preparation method therefor, and use thereof

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